ASTM D7979-17
(Test Method)Standard Test Method for Determination of Per- and Polyfluoroalkyl Substances in Water, Sludge, Influent, Effluent and Wastewater by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS)
Standard Test Method for Determination of Per- and Polyfluoroalkyl Substances in Water, Sludge, Influent, Effluent and Wastewater by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS)
SIGNIFICANCE AND USE
5.1 PFASs are widely used in various industrial and commercial products; they are persistent, bio-accumulative, and ubiquitous in the environment. PFASs have been reported to exhibit developmental toxicity, hepatotoxicity, immunotoxicity, and hormone disturbance. A draft Toxicological Profile for Perfluoroalkyls from the U.S. Department of Health and Human Services is available.6 PFASs have been detected in soils, sludges, surface, and drinking waters. Hence, there is a need for quick, easy, and robust method to determine these compounds at trace levels in water matrices for understanding of the sources and pathways of exposure.
5.2 This method has been investigated for use with reagent, surface, sludge and wastewaters for selected PFASs. This method has not been evaluated on drinking water matrices.
SCOPE
1.1 This procedure covers the determination of selected per- and polyfluoroalkyl substances (PFASs) in a water matrix using liquid chromatography (LC) and detection with tandem mass spectrometry (MS/MS). These analytes are qualitatively and quantitatively determined by this method. This method adheres to a technique known as selected reaction monitoring (SRM) or sometimes referred to as multiple reaction monitoring (MRM). This is not a drinking water method, performance of this test method has not been evaluated on drinking water matrices.
1.2 The Method Detection Limit (MDL)2 and Reporting Range3 for the target analytes are listed in Table 1. The target concentration for the reporting limit for this test method was 10 ng/L for most of the target analytes at the time of development.
TABLE 1 Method Detection Limit and Reporting Range
AnalyteA
MDL
(ng/L)
Reporting Ranges
(ng/L)
PFTreAB
1.2
10 – 400
PFTriAB
0.7
10 – 400
PFDoAB
1.2
10 – 400
PFUnAB
1.2
10 – 400
PFDAB
1.4
10 – 400
PFOSB
2.2
10 – 400
PFNAB
1.1
10 – 400
PFecHSB
1.9
10 – 400
PFOAB
1.7
10 – 400
PFHxSB
1.2
10 – 400
PFHpAB
1.0
10 – 400
PFHxAB
2.0
10 – 400
PFBSB
0.8
10 – 400
PFPeAB
4.6
50 – 2000
PFBAB
4.6
50 – 2000
FHEA
92.9
300 – 8000
FOEA
106.8
300 – 8000
FDEA
47.2
200 – 8000
FOUEA
2.3
10 – 400
FHpPA
3.3
10 – 400
FHUEA
1.5
10 – 400(A) Acronyms are defined in 3.3.(B) New MDL study was reported in August 2016, which resulted in a reporting limit and range update.
1.2.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. The reporting limit may be lowered providing your lab meets the minimum performance requirements of this test method at the lower concentrations, this method is performance based and modifications are allowed to improve performance. Analyte detections between the method detection limit and the reporting limit are estimated concentrations and are not reported following this test method. In most cases, the reporting limit is the concentration of the Level 1 calibration standard as shown in Table 4 for the PFASs after taking into account the 50 % dilution with methanol. It is above the Level 1 calibration concentration for FHEA and FOEA, these compounds can be identified at the Level 1 concentration but the standard deviation among replicates at this lower spike level resulted in a higher reporting limit.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principle...
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Designation:D7979 −17
Standard Test Method for
Determination of Per- and Polyfluoroalkyl Substances in
Water, Sludge, Influent, Effluent and Wastewater by Liquid
1
Chromatography Tandem Mass Spectrometry (LC/MS/MS)
This standard is issued under the fixed designation D7979; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope identified at the Level 1 concentration but the standard devia-
tion among replicates at this lower spike level resulted in a
1.1 Thisprocedurecoversthedeterminationofselectedper-
higher reporting limit.
and polyfluoroalkyl substances (PFASs) in a water matrix
using liquid chromatography (LC) and detection with tandem 1.3 The values stated in SI units are to be regarded as
mass spectrometry (MS/MS). These analytes are qualitatively standard. No other units of measurement are included in this
and quantitatively determined by this method. This method standard.
adheres to a technique known as selected reaction monitoring
1.4 This standard does not purport to address all of the
(SRM) or sometimes referred to as multiple reaction monitor-
safety concerns, if any, associated with its use. It is the
ing (MRM).This is not a drinking water method, performance
responsibility of the user of this standard to establish appro-
of this test method has not been evaluated on drinking water
priate safety, health and environmental practices and deter-
matrices.
mine the applicability of regulatory limitations prior to use.
2
1.5 This international standard was developed in accor-
1.2 The Method Detection Limit (MDL) and Reporting
3
dance with internationally recognized principles on standard-
Range for the target analytes are listed in Table 1. The target
ization established in the Decision on Principles for the
concentrationforthereportinglimitforthistestmethodwas10
Development of International Standards, Guides and Recom-
ng/Lformostofthetargetanalytesatthetimeofdevelopment.
mendations issued by the World Trade Organization Technical
1.2.1 Thereportinglimitinthistestmethodistheminimum
Barriers to Trade (TBT) Committee.
value below which data are documented as non-detects. The
reporting limit may be lowered providing your lab meets the
2. Referenced Documents
minimum performance requirements of this test method at the
4
lower concentrations, this method is performance based and
2.1 ASTM Standards:
modifications are allowed to improve performance. Analyte
D1129Terminology Relating to Water
detections between the method detection limit and the report-
D1193Specification for Reagent Water
ing limit are estimated concentrations and are not reported
D2777Practice for Determination of Precision and Bias of
following this test method. In most cases, the reporting limit is
Applicable Test Methods of Committee D19 on Water
the concentration of the Level 1 calibration standard as shown
D3856Guide for Management Systems in Laboratories
in Table 4 for the PFASs after taking into account the 50 %
Engaged in Analysis of Water
dilution with methanol. It is above the Level 1 calibration
D3694Practices for Preparation of Sample Containers and
concentration for FHEA and FOEA, these compounds can be
for Preservation of Organic Constituents
D4841Practice for Estimation of Holding Time for Water
Samples Containing Organic and Inorganic Constituents
1
This test method is under the jurisdiction ofASTM Committee D19 on Water
D5847Practice for Writing Quality Control Specifications
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
Organic Substances in Water.
for Standard Test Methods for Water Analysis
Current edition approved July 15, 2017. Published August 2017. Originally
E2554Practice for Estimating and Monitoring the Uncer-
approved in 2015. Last previous edition approved in 2016 as D7979–16. DOI:
tainty of Test Results of a Test Method Using Control
10.1520/D7979-17.
2
Chart Techniques
The MDLis determined following the Code of Federal Regulations (CFR) , 40
CFR Part 136, Appendix B utilizing dilution and filtration. 5 mL sample of water
was utilized.Adetailed process determining the MDLis explained in the reference
and is beyond the scope of this test method to be explained here.
3 4
Reporting range concentration is calculated from Table 4 concentrations For referenced ASTM standards, visit the ASTM website, www.astm.org, or
assuming a 30 µL injection of the Level 1 calibration standard for PFASs, and the contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
highestlevelcalibrationstandardwitha10mLfinalextractvolumeofa5mLwater Standards volume information, refer to the standard
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D7979 − 16 D7979 − 17
Standard Test Method for
Determination of Perfluorinated Compounds Per- and
Polyfluoroalkyl Substances in Water, Sludge, Influent,
Effluent and Wastewater by Liquid Chromatography Tandem
1
Mass Spectrometry (LC/MS/MS)
This standard is issued under the fixed designation D7979; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This procedure covers the determination of selected perfluorinated compounds (PFCs) per- and polyfluoroalkyl substances
(PFASs) in a water matrix using liquid chromatography (LC) and detection with tandem mass spectrometry (MS/MS). These
analytes are qualitatively and quantitatively determined by this method. This method adheres to a technique known as selected
reaction monitoring (SRM) or sometimes referred to as multiple reaction monitoring (MRM) mass spectrometry.(MRM). This is
not a drinking water method, performance of this test method has not been evaluated on drinking water matrices.
2 3
1.2 The Method Detection Limit (MDL) and Reporting Range for the target analytes are listed in Table 1. The target
concentration for the reporting limit for this test method was 10 ng/L for most of the target analytes at the time of development.
1.2.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. The
reporting limit may be lowered providing your lab meets the minimum performance requirements of this test method at the lower
concentrations, this method is performance based and modifications are allowed to improve performance. Analyte detections
between the method detection limit and the reporting limit are estimated concentrations and are not reported following this test
method. In most cases, the reporting limit is the concentration of the Level 1 calibration standard as shown in Table 4 for the
perfluorinated compounds PFASs after taking into account the 50 % dilution with methanol. It is above the Level 1 calibration
concentration for PFOS, PFBS, FHEA and FOEA, these compounds can be identified at the Level 1 concentration but the standard
deviation among replicates at this lower spike level resulted in a higher reporting limit.
1.3 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this
standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
4
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
1
This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
Organic Substances in Water.
Current edition approved June 1, 2016July 15, 2017. Published June 2016August 2017. Originally approved in 2004.2015. Last previous edition approved in 20152016
ε1
as D7979 – 15D7979 – 16. . DOI: 10.1520/D7979-16.10.1520/D7979-17.
2
The MDL is determined following the Code of Federal Regulations, Regulations (CFR) , 40 CFR Part 136, Appendix B utilizing dilution and filtration. 5 mL sample
of water was utilized. A detailed process determining the MDL is explained in the reference and is beyond the scope of this test method to be explained here.
3
Reporting range concentration is calculated from Table 4 concentrations assuming a 30 μL injection of the Level 1 calibration standard for PFCs,PFASs, and the highest
level calibration standard with a 10 mL final extract volume of a 5 mL water sample. Volume variations will change the reporting limit and ranges.
4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
...
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